Pectin product and process of



Reiseued June 5, 1934 PATENT OFFICE 1am. rsc'rnz raonuc'r m raocsss or PRODUCING SAME Eloise Jameson, Corona,.Calif., assignor to California Fruit Growers Exchange, Los Angeles, Calif., a corporation of California No Drawing. Original No. 1,611,528. dated Deoember 21, 1926, Serial No. 63,132, October 17, 1925. Application for reissue May 28, 1932,

Serial No. 613,139

27 Claims. (CI. 99-11) In the preparation of pectin from different sources such as apple pomace, citrus fruit pulp, beet' pulp, etc., various methods of extracting pectin are used and various methods of purifying the pectic solution or of separating the pectin from the solution by drying, precipitation, etc., may be used.

As a result of variations in the process of extraction, isolation, or purification of the pectin, I have discovered that the pectin product may not be uniform as to its acid character. This may be due to the acidity of the pectic substance itself or to the acidity of the product on account of the presence of some added acid remaining as an impurity after certain steps in the commercial process or to both such causes.

The expression pH as here used means the pH of a solution made up as follows: 0.5 gram of the pectin preparation is moistened with 1 cc. 0% strong alcohol and then, dissolved in .100 cc. 0 water. The pH is determined colorimetrically on this solution. r

I have found that unless the acidity of the preparation falls within certain limits as pH 3.4 to pH 7.0 the pectic preparation is not satisfactory for jelly making. The percentage of total acid is not the important point but rather the concentration of hydrogen ions or as it is now usually'expressed the pH value. I

I have found that for ins ance if a pectin preparation having a pH of 3.2 is. used to make commercial Jelly no jelly can be made since it will set in the cooking kettle before it can be poured. If we treat the pectin so as to make the pH 3.7 and then proceed to make the Jelly just as before we will produce a perfect commercial jelly.

Now insome pectin preparations where a" strong acid such as hydrochloric acid has been used to reduce the mineral ash content of the pectin and a very small amount of HCl is left in the product the pH will be low as for instance 2.6 and such a pectin is not satisfactory for jelly making purposes.

In U. 8. Patent No. 1,497,884 there is described a process for the removal of the free HCl with neutral alcohol. This is an expensive and sometimes difllcult process and does-not admit of as accurate or convenient control of the pectin as does the method herein disclosed.

This invention consists in the adjustment of the pH to the desired point in either of two ways but the underlying chemical principle is the same; namely, that if the salt of a strong base and a weak acid is introduced in proper amount the strong base will combine with the strong acid that is thecause of the low pH value of the pectin and will set free the weak acid which on account of its smaller dissociation constant causes the pH of the pectin preparation to be raised to the de- 60 sired point.

The proportions of the base and the acid making up the. salt should be such that the salt elapsed for the reactions to take'place the pectin is separated from the solution by means of a filter press or other convenient means. The pec tin may be washed with alcohol and dried wh it is ready for use.

2nd. The powdered pectin may be mixed with a proper amount of the dry salt of a strong base and a weak acid as sodium citrate, sodium carbonate, sodium acetate, etc., so that when the resulting pectin preparation is dissolved the pH will fall within the range pH 3.4 to pH 7.0.

I have found also that if-the original somewhat impure pectin preparation, before being washed with the alcoholic HCl, is mixed with the proper 1 proportion of an organic acid such as'citrlc acid or tartaric acid and a salt of a strong baseand a weak acid such as sodium acetate or sodium bicarbonate the pectin is quite readily put into solution and is properly standardized as to pH.

The use of a carbonate or a bicarbonate 'is advantageous here as the liberation of C0: assists materially in dispersing the pectin particles thus bringing each particle into contact with the solution so that the formationof lumps is avoided and the preparation goes readily into; solution.

As a result of the application of this invention I am able to produce a pectin preparation of any desired predetermined pH and thus insure uniformly satisfactory results in the use of the pectin.

Further by the selecting of pectin preparations of varying Jellying strength we are able to standardize the product so that each pound of the final pectin preparation will produce satisfactory Jelly with a definite amount of sugar.

Atypical use of' this invention is-as follows:

'Pectinisproducedi'rom any satistactorysource such as apple pomace, citrus fruit pulp, etc., by -the method described in U. 8. Patent No. 1,497,884

or by some other suitable method.

economicaltowashoutallthehydrochloricacid thathasbeenusedinslishtexcessi'ortheremoval of aluminum, calcium orother mineral impurities. We may assume then that we have a dry powdered pectin preparation that contains enough strong acid such as hydrochloric acid to brin: thepH value to a point below 3.4 which we have found is the minimum for producing satisi'actory Jellies.

It sometimes happens that it is dimcult or unll In accordance with this invention we may' pro-,

eeedineitheroi'twowaystobringthepectin prepsrationwithinthepnranze oi 3.4to'L0 whichlhavei'oundarethelimitingvaluesior apectinpreparationtobeusediormakinaielly intheusualmannereitherwithcanesugaror with lucose. a

' Inthepracticeotmyinventionthedrypectin preparation is ground to a fine powder and is in alcohol 01! preferably about -95%stren3thinwhichis dissolved or suspended suflicient sodium acetate or sodium citrateorothersaltoiastronsbaseandaweak sodium acetate, sodium carbonate, sodium' bicarbonate, etc; It is of course important in using such salts as carbonates and bicarbonates that the preparation be to become alkabubhles is oimateriai in pectin into solution since the as to separate the individuaipectin preventinttheiormationoilumps juice or water to reach andaliowinstheacid each particle so that solution is readily eiiected. Amountoi salttohe added-'isdetermined by suspending a known weight'oi pectin in strona much more readily soluble than the originalpecsaltaddedisabout% to%oftheamount necessary as indicated by the titration.

The preparation made by the addition of the neutralsalttotheoriginalpectinproductis tin product.

As aresultofthismixlnsoi'thepectinm' aration and neutral salt or both the salt and dry organic acid there is obtained a pectin preparationoideiinite pHandturther-inpractice I mixseverallotsotpectinoivm sleilying powersothat lpartbyweightottheiinal product will iali 140,160, 200 or other definite predetermined number of parts by weight. of sugar in making'regular jelly either with-cane sugar or with glucose. I

Having fully described my said invention what I claim is:

701. A dry pectin producthavina apHot 3.4 to

2. A pectinproduct which is a mixture 0! an original-pectin product with asaltoi a strona baseandaweakacidplaced in an'acid solution the ionna-.

3.'A soluble pectin product whichisa mixture or anoriginal water-insoluble pectinpreparation. adryorgsnicacidandasaltoiastronsbaseand anacidweakerthanthedryorganicacidinsuch proportions that the pH of the mixture lies between 34 and 7.0.

4. A pectin product which is a mixture of an'-1 05 orizinaipectinpreparationwithasaltoiastrona baseandaweakacidinsuchproportionsthatthe pI-IoithemixtureliesbetweenBAand'm.

5. Animprovementintheprocess'oiproduciny pectinwhichconsistsinaddinstoapectinmrationwhichisnot oiproperpliasaltoiastron: baseandaweakacidin'suchproportionsthatthe nnishedproducthasapfloiaato'lli.

8.Animprovementintheprocessoiproducinz v pectinwhichconsistsinwashingcrudeorpartlyllfi purifledpectinwith asolution (preterablyinal-- coholoi'properstrenzth) oiasaltotastrona baseandaweakacidsothatanexchanzeisebiectedinwhichthestrongbaselmiteswiththe strongacidwhichmayexistasanimpurityinlflfl theoriginalpectin preparation andthereby form asaltoithestronzbaseandthestronaacidleavingaweakacidinplaceoithestronzonathus brinzinathepl-ioi'thepectinpmtiontoany predetermined point.

'i. An improvementintheprocessoiproducinz pectinwhichconsistsinaddingtoapectinpreparationwhichhasnotbeensubiectedtoanacidalcoholwashamixtureoianorsanicacidwitha saltotastmnabaseandanacidweakerthanthem oraanicacidusedinsuchproportionth'atthennishedpfoductissolubleandhasapHoISAto'LO.

8. A dry pectin preparation containingv a car bonateorabicarbonate. A I

9. Adrypectin product containins aneflervescentsaltoiastronsbaseanda'weakacidi 'taininapectin; acarbonate orabicarbonate and 10.Asolublepectinproductwhichisa nixture of an original pectin preparation withan enervescentsaltoi'astronabaseandaweakacidin suchthatthepfloithemixtm'elieslm betweentiand'm. 11. Aiinelydividedpectinpreparationcontain-q ingpectinands teorabicarbonate.

12.Aiineiy di pectin preparation conadrrorzanicacid. 13.As\ibltflitlll] dry.iinelydividedpect in ILA iinely divided preparation containing pectin, an efiervescent salt of a strong base and a weak acid, and a dry organic acid.

15. A finely divided, pectin preparation containing pectin, an eflervescent salt of a strong baseand a weak acid, and fineLy divided citri acid.

16. A soluble gum composition consisting of a citrus pectin containing substance difilcultly soluble in boiling water, sodium bicarbonate and citric acid in slight excess.

17. A soluble pectin product containing pectin difilcultly soluble in water, an efiervescent salt of a strong base and a weak acid, and a dry organic acid in a quantity at least suificient to decompose the effervescent salt.

18. A soluble pectin product containing pectin, a carbonate or a bicarbonate, and a dry organic acid in quantity slightly in excessoi' that required to decompose the carbonate or bicarbonate.

19. The method of dispersing and dissolving difllcultly soluble pectin which comprises mixing the pectin with an efiervescent salt oi a strong base and a weak acid and a dry organic acid in a quantity at least sufilcient to decompose the effervescent salt, and placing the mixture in an aqueous medium whereby, through the interaction of the organic acid and the salt, efiervescence is produced and thepectin is there-'- by dispersed in the aqueous medium and its solution facilitated.

Reissue No. 19,197.

ELOISE JAMESON.

20. The method of dispersing and dissolving dlmcultly soluble pectin which comprises placing in an aqueous medium a mixture of the pectin with an eil'ervescent salt 01 a strong base and a weak acid and a dry organic acid whereby, through the interaction of the organic acid and the salt, efiervescence is produced and the pectin is dispersed in the aqueous medium and its solution facilitated.

21. A pectin product which is a mixture of pectin with a, salt oi a strong base and a weak acid in such proportions that the pH 01 the mixture lies between 3.4 and 7.0.

22. A finely divided pectin preparation containing pectin and sodium acetate.

23. A finely divided pectin preparation con taining pectin and sodium citrate.

24. A finely divided pectin preparation containing pectin, sodium acetate and a dry organic acid. I l

25. A dry pectin product containing sodium acetate, said product having a pH of 3.4 to 7.0.

26. A dry pectin product containing sodium citrate, said product having a pH of 3.4 to 7.0.

27. A pectin product adapted for use in the manufacture of commercial Jellies, comprising a dry mixture of pectin and a salt 01 a strong base and a weak acid.

nnorsr: JAMESON.

. June 5, 4--

It is hereby certified that error appears in the printed specification of the above ninnbered patent requiring correction as follows: Page 1, first column, lino I 5, strike out the word "neutral"; and that the said Letters Patent should'be read with this correctiontherein that the same'nay con- (form to the record of -'the ca 5 s in the Patent Office, A

Signed sealed this 8th day or March; A. D; 1938.,

(Soul) Henry Van Arsdale, Acting Commissioner of Patents.

its

preparation containing pectin, an efiervescent salt of a strong base and a weak acid, and a dry organic acid.

15. A finely divided, pectin preparation containing pectin, an eflervescent salt of a strong baseand a weak acid, and fineLy divided citri acid.

16. A soluble gum composition consisting of a citrus pectin containing substance difilcultly soluble in boiling water, sodium bicarbonate and citric acid in slight excess.

17. A soluble pectin product containing pectin difilcultly soluble in water, an efiervescent salt of a strong base and a weak acid, and a dry organic acid in a quantity at least suificient to decompose the effervescent salt.

18. A soluble pectin product containing pectin, a carbonate or a bicarbonate, and a dry organic acid in quantity slightly in excessoi' that required to decompose the carbonate or bicarbonate.

19. The method of dispersing and dissolving difllcultly soluble pectin which comprises mixing the pectin with an efiervescent salt oi a strong base and a weak acid and a dry organic acid in a quantity at least sufilcient to decompose the effervescent salt, and placing the mixture in an aqueous medium whereby, through the interaction of the organic acid and the salt, efiervescence is produced and thepectin is there-'- by dispersed in the aqueous medium and its solution facilitated.

Reissue No. 19,197.

ELOISE JAMESON.

20. The method of dispersing and dissolving dlmcultly soluble pectin which comprises placing in an aqueous medium a mixture of the pectin with an eil'ervescent salt 01 a strong base and a weak acid and a dry organic acid whereby, through the interaction of the organic acid and the salt, efiervescence is produced and the pectin is dispersed in the aqueous medium and its solution facilitated.

21. A pectin product which is a mixture of pectin with a, salt oi a strong base and a weak acid in such proportions that the pH 01 the mixture lies between 3.4 and 7.0.

22. A finely divided pectin preparation containing pectin and sodium acetate.

23. A finely divided pectin preparation con taining pectin and sodium citrate.

24. A finely divided pectin preparation containing pectin, sodium acetate and a dry organic acid. I l

25. A dry pectin product containing sodium acetate, said product having a pH of 3.4 to 7.0.

26. A dry pectin product containing sodium citrate, said product having a pH of 3.4 to 7.0.

27. A pectin product adapted for use in the manufacture of commercial Jellies, comprising a dry mixture of pectin and a salt 01 a strong base and a weak acid.

nnorsr: JAMESON.

. June 5, 4--

It is hereby certified that error appears in the printed specification of the above ninnbered patent requiring correction as follows: Page 1, first column, lino I 5, strike out the word "neutral"; and that the said Letters Patent should'be read with this correctiontherein that the same'nay con- (form to the record of -'the ca 5 s in the Patent Office, A

Signed sealed this 8th day or March; A. D; 1938.,

(Soul) Henry Van Arsdale, Acting Commissioner of Patents.

its 

